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A validated chiral LC method for the enantiomeric separation of AT13148 on polysaccharide-based chiral stationary phase

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Abstract

A sensitive and accurate LC method for the determination of AT13148 enantiomeric purity has been developed and validated. Baseline separation with a resolution higher than 1.8 was accomplished within 15 min using a Chiralpak AD-H column (250 × 4.6 mm; particle size 5 μm) and n-hexane: 2-propanol: diethylamine (85:15:0.1, v/v) as mobile phase at a flow rate of 1 mL min−1. Eluted analytes were monitored by UV absorption at 254 nm. The effects of mobile phase components, temperature and flow rate on enantiomeric selectivity and resolution of enantiomers were investigated. Calibration curves were plotted within the concentration range between 7 and 500 μg mL−1 (n = 11), and the recoveries between 98.24 and 100.99% were obtained, with relative standard deviation lower than 1.32%. LOD and LOQ for AT13148 were 2.46 and 7.38 μg mL−1 and for its enantiomer were 2.54 and 7.49 μg mL−1, respectively. It was demonstrated that the developed method was accurate, robust and sensitive for the determination of enantiomeric purity of AT13148, especially for the analysis of bulk samples.

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Acknowledgements

This study was funded by the National Natural Science Foundation of China (No. 81602950) and Health and Family Planning Commission of Sichuan Province Scientific Research Project (No. 17PJ558).

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Author notes

  1. Yong Xia and Zhihao Liu have contributed equally to this work.

Authors and Affiliations

  1. Cancer Center, West China Hospital, Sichuan University and Collaborative Innovation Center, Chengdu, 610041, China

    Yong Xia, Zhihao Liu, Yiwen Zhang & Xuelei Ma

  2. Sichuan Taihuatang Pharmaceutical Co., Ltd, No. 18, Section 4, Nanchang Road, Guanghan, 618300, China

    Yong Huang

  3. Department of Hepatobiliary and Pancreas Surgery, Second Clinical Medical College of Jinan University (Shenzhen People’s Hospital), Shenzhen, 518020, China

    Xiaojun Huang

  4. Sichuan Nursing Vocational College, Chengdu, 610100, China

    Mengya Liao

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  1. Yong Xia
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  2. Zhihao Liu
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  3. Yong Huang
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  4. Xiaojun Huang
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Correspondence to Yiwen Zhang or Xuelei Ma.

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Xia, Y., Liu, Z., Huang, Y. et al. A validated chiral LC method for the enantiomeric separation of AT13148 on polysaccharide-based chiral stationary phase. J IRAN CHEM SOC 15, 711–717 (2018). https://doi.org/10.1007/s13738-017-1270-2

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  • DOI: https://doi.org/10.1007/s13738-017-1270-2

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